#------------------------------------------------------------------------------ #$Date: 2020-05-06 22:20:40 +0300 (Wed, 06 May 2020) $ #$Revision: 251821 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/83/4038331.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4038331 loop_ _publ_author_name 'Chen, Chien-Tien' 'Maity, Nabin Ch' 'Agarwal, Rachit' 'Lai, Chien-Fu' 'Liao, Yiya' 'Yu, Wei-Ru' _publ_section_title ; Chiral Vanadyl(V) Complexes Enable Efficient Asymmetric Reduction of \b-Ketoamides: Application toward (S)-Duloxetine. ; _journal_name_full 'The Journal of organic chemistry' _journal_paper_doi 10.1021/acs.joc.0c00221 _journal_year 2020 _chemical_formula_sum 'C8 H11 N O2 S' _chemical_formula_weight 185.24 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/6 _cell_angle_alpha 90 _cell_angle_beta 99.936(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.1326(9) _cell_length_b 15.291(2) _cell_length_c 8.2001(12) _cell_measurement_reflns_used 4353 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 26.3458 _cell_measurement_theta_min 2.6641 _cell_volume 880.9(2) _computing_cell_refinement 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 8.3333 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_unetI/netI 0.0206 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 7088 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.356 _diffrn_reflns_theta_min 2.664 _exptl_absorpt_coefficient_mu 0.325 _exptl_absorpt_correction_T_max 0.9485 _exptl_absorpt_correction_T_min 0.8815 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2014/4 (Bruker AXS Inc.)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description tabullar _exptl_crystal_F_000 392 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.386 _refine_diff_density_min -0.293 _refine_diff_density_rms 0.056 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 111 _refine_ls_number_reflns 1784 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.077 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0325 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+0.6760P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0875 _refine_ls_wR_factor_ref 0.0896 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1646 _reflns_number_total 1784 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jo0c00221_si_002.cif _cod_data_source_block 161236LT_0m _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_crystal_density_meas' value 'not measured' was changed to '?' -- the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 4038331 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelxl_version_number 2014/6 _shelx_res_file ; TITL 161236LT_0m in P2(1)/c CELL 0.71073 7.1326 15.2912 8.2001 90.000 99.936 90.000 ZERR 4.00 0.0009 0.0021 0.0012 0.000 0.004 0.000 LATT 1 SYMM -x, y+1/2, -z+1/2 SFAC C H N O S UNIT 32 44 4 8 4 L.S. 4 ACTA BOND $H FMAP 2 PLAN 5 TEMP -173.000 WGHT 0.042500 0.676000 FVAR 1.02361 S1 5 0.552580 -0.155313 0.118405 11.00000 0.02200 0.01520 = 0.01382 -0.00174 0.00293 -0.00310 O1 4 0.726982 -0.066611 0.467222 11.00000 0.01224 0.01530 = 0.01136 0.00274 0.00224 -0.00075 AFIX 147 H5 2 0.635713 -0.096596 0.488914 11.00000 -1.50000 AFIX 0 O2 4 0.601243 0.148689 0.517295 11.00000 0.01162 0.01669 = 0.02118 -0.00280 0.00386 0.00024 N1 3 0.921458 0.149718 0.590186 11.00000 0.01116 0.01569 = 0.01832 -0.00482 0.00192 0.00147 AFIX 43 H8 2 1.030663 0.130739 0.567718 11.00000 -1.20000 AFIX 0 C1 1 0.923056 0.206613 0.732436 11.00000 0.01849 0.02360 = 0.02412 -0.01170 0.00133 0.00135 AFIX 137 H1 2 0.792058 0.221995 0.742157 11.00000 -1.50000 H9 2 0.994545 0.259962 0.717980 11.00000 -1.50000 H10 2 0.983643 0.176239 0.833073 11.00000 -1.50000 AFIX 0 C2 1 0.761087 0.125203 0.492542 11.00000 0.01441 0.00941 = 0.01536 0.00175 0.00407 -0.00080 C3 1 0.784872 0.070343 0.344135 11.00000 0.01459 0.01307 = 0.01364 -0.00032 0.00324 -0.00155 AFIX 23 H11 2 0.920007 0.052827 0.354220 11.00000 -1.20000 H7 2 0.752072 0.106211 0.242712 11.00000 -1.20000 AFIX 0 C4 1 0.661361 -0.011259 0.326497 11.00000 0.01117 0.01205 = 0.01104 0.00059 0.00131 0.00034 AFIX 13 H6 2 0.526363 0.005955 0.327764 11.00000 -1.20000 AFIX 0 C5 1 0.671932 -0.057878 0.165920 11.00000 0.01090 0.01205 = 0.01321 -0.00029 -0.00025 0.00103 C6 1 0.766789 -0.033130 0.039472 11.00000 0.01319 0.01528 = 0.01168 -0.00126 -0.00001 0.00066 AFIX 43 H4 2 0.840690 0.018646 0.041031 11.00000 -1.20000 AFIX 0 C7 1 0.740333 -0.094702 -0.093615 11.00000 0.01883 0.02748 = 0.01211 -0.00089 0.00348 0.00294 AFIX 43 H2 2 0.794609 -0.088003 -0.190841 11.00000 -1.20000 AFIX 0 C8 1 0.629742 -0.163763 -0.067032 11.00000 0.02235 0.02054 = 0.01351 -0.00473 -0.00059 0.00245 AFIX 43 H3 2 0.599054 -0.210956 -0.142248 11.00000 -1.20000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM 161236LT_0m in P2(1)/c REM R1 = 0.0325 for 1646 Fo > 4sig(Fo) and 0.0351 for all 1784 data REM 111 parameters refined using 0 restraints END WGHT 0.0424 0.6785 REM Highest difference peak 0.386, deepest hole -0.293, 1-sigma level 0.056 Q1 1 0.7523 -0.0608 -0.0202 11.00000 0.05 0.39 Q2 1 1.0501 0.2158 0.7851 11.00000 0.05 0.36 Q3 1 0.7675 0.0977 0.4138 11.00000 0.05 0.36 Q4 1 0.6016 -0.1611 0.0154 11.00000 0.05 0.35 Q5 1 0.6212 -0.0983 0.1493 11.00000 0.05 0.33 ; _shelx_res_checksum 92179 _shelx_hkl_file ; 2 0 0 1728.63 41.8297 1 2 0 0 1726.46 41.7680 1 2 0 0 1668.96 43.6540 3 3 0 0 425.726 11.5926 1 3 0 0 414.543 10.8662 1 4 0 0 255.729 7.51800 2 4 0 0 252.066 7.29218 1 4 0 0 264.577 8.51402 1 5 0 0 10.1165 1.31956 2 5 0 0 10.6345 2.03022 1 5 0 0 10.5981 1.31612 1 6 0 0 1639.56 41.0718 1 6 0 0 1677.68 44.0216 1 6 0 0 1595.03 41.1688 2 7 0 0 69.3376 5.42769 1 8 0 0 53.5796 6.09220 1 0 -1 0 -2.0191 0.06673 1 0 -1 0 -1.8356 0.06906 2 0 -1 0 -1.8422 0.13623 1 0 1 0 -2.0071 0.06010 1 0 1 0 -2.0132 0.10819 1 0 1 0 -1.8499 0.07382 2 1 -1 0 31.1598 2.15875 1 -1 -1 0 34.8497 1.47760 3 1 -1 0 35.8215 1.81125 1 1 1 0 31.4065 1.45670 3 1 1 0 33.4953 1.35481 1 1 1 0 35.9296 1.47056 1 -1 1 0 35.4615 2.10654 1 -2 -1 0 4801.92 118.540 3 2 -1 0 4981.47 120.419 1 2 -1 0 4730.63 121.539 1 2 1 0 4772.06 115.982 1 2 1 0 4814.71 118.281 3 2 1 0 4748.27 116.364 1 3 -1 0 90.3119 3.22745 1 3 -1 0 87.9307 4.04045 1 3 1 0 85.8344 2.64219 1 3 1 0 80.4612 3.13623 2 3 1 0 87.2529 3.01683 1 4 -1 0 540.392 13.8411 2 4 -1 0 514.925 14.2142 1 4 -1 0 558.943 16.0171 1 4 1 0 512.373 14.2682 2 4 1 0 521.204 13.6142 1 4 1 0 537.779 14.6292 1 5 -1 0 70.5752 3.24178 1 5 -1 0 69.6793 2.91632 2 5 -1 0 72.3775 4.61306 1 5 1 0 71.3892 3.27757 2 5 1 0 66.4844 2.79909 1 5 1 0 66.3018 3.87422 1 6 -1 0 769.864 22.9569 1 6 -1 0 705.890 19.7108 1 6 -1 0 723.463 19.2084 2 6 1 0 742.437 21.5946 1 6 1 0 698.986 19.7653 2 6 1 0 726.359 19.1366 1 7 -1 0 359.955 14.5343 1 7 1 0 360.612 13.4801 1 8 -1 0 3.69644 2.12837 1 8 1 0 -2.6358 1.35679 1 0 -2 0 1280.83 33.4676 1 0 -2 0 1302.68 33.1518 1 0 -2 0 1299.64 32.4079 2 0 2 0 1239.28 32.1180 1 0 2 0 1245.99 31.8370 2 1 -2 0 76.8853 1.98093 2 1 -2 0 75.9010 3.68236 1 -1 -2 0 76.3557 2.51675 1 1 2 0 70.8188 2.34867 1 -1 2 0 76.7801 2.97616 1 1 2 0 76.3454 2.68542 1 -1 2 0 68.7500 3.47664 1 2 -2 0 8816.25 217.597 1 -2 -2 0 8649.48 212.354 3 2 -2 0 8975.07 224.592 1 2 2 0 8621.07 213.513 1 -2 2 0 8637.53 215.556 1 -3 -2 0 241.724 6.85440 3 3 -2 0 249.208 9.01048 1 3 -2 0 251.336 7.63713 1 3 2 0 248.048 7.36436 2 3 2 0 240.368 6.54989 1 3 2 0 242.207 7.04267 1 4 -2 0 690.714 18.7347 1 4 -2 0 690.275 17.5458 2 4 -2 0 695.751 20.8598 1 4 2 0 714.834 17.6144 1 4 2 0 692.666 18.5784 2 4 2 0 704.906 18.5777 1 5 -2 0 44.6353 2.75421 1 5 -2 0 48.1180 4.85984 1 5 -2 0 48.3274 2.11460 2 5 2 0 43.9590 3.00698 1 5 2 0 46.6220 2.68826 2 5 2 0 42.0731 2.06654 1 6 -2 0 155.171 8.29859 1 6 -2 0 139.545 4.76821 2 6 -2 0 133.313 5.69915 1 6 2 0 146.923 6.72072 1 6 2 0 137.556 4.87832 1 7 -2 0 22.6444 4.22030 1 7 2 0 23.5671 3.28173 1 8 -2 0 61.8901 7.18053 1 8 2 0 69.4129 5.61778 1 0 -3 0 -3.9519 0.29475 1 0 -3 0 -3.3283 0.56124 1 0 3 0 -3.1825 0.51450 1 0 3 0 -3.0664 0.28578 2 0 3 0 -3.5597 0.32601 1 1 -3 0 2259.49 55.3043 2 1 -3 0 2233.06 56.7295 1 -1 -3 0 2211.80 55.5439 1 -1 3 0 2230.13 55.0616 2 1 3 0 2146.72 56.5653 1 1 3 0 2257.38 56.7360 2 1 3 0 2247.36 58.3459 1 -1 3 0 2223.33 55.0961 1 2 -3 0 582.797 18.3034 1 2 -3 0 607.273 16.7202 1 -2 -3 0 628.345 15.0748 1 -2 -3 0 609.369 15.5030 3 2 -3 0 613.817 14.7647 2 2 3 0 620.015 15.5520 1 2 3 0 618.067 16.0379 2 2 3 0 610.182 16.1343 1 3 -3 0 298.410 10.8844 1 -3 -3 0 275.845 7.82264 3 3 -3 0 277.721 8.93968 1 3 3 0 272.274 8.33531 1 3 3 0 286.210 7.70894 1 3 3 0 290.395 8.51990 2 -3 3 0 289.342 8.60178 1 -4 -3 0 570.220 14.9595 3 4 -3 0 565.411 16.1458 1 4 -3 0 564.572 18.5497 1 4 -3 0 568.154 14.1418 2 4 3 0 542.729 15.6247 1 4 3 0 585.485 14.6852 1 4 3 0 576.578 15.7732 2 5 -3 0 81.4841 2.74984 2 5 -3 0 77.6098 5.78763 1 5 -3 0 78.6758 4.09716 1 5 3 0 79.8717 3.12362 1 5 3 0 84.5362 4.28181 1 6 -3 0 380.667 15.2182 1 6 3 0 341.011 12.2035 1 6 3 0 364.614 10.3008 1 7 -3 0 15.5372 3.69342 1 7 3 0 26.0249 3.60462 1 8 -3 0 3.74368 2.51950 1 8 3 0 9.07734 2.44615 1 0 -4 0 6898.09 177.303 1 0 4 0 7265.89 173.841 2 0 4 0 6953.85 176.999 1 0 4 0 7006.79 177.795 1 1 -4 0 1475.35 41.6505 1 1 -4 0 1557.19 39.7501 1 -1 -4 0 1526.43 40.1865 1 1 -4 0 1497.91 39.0646 1 1 -4 0 1577.57 39.6191 2 -1 4 0 1554.25 39.8767 1 -1 4 0 1600.08 39.0583 2 1 4 0 1654.52 39.6178 1 1 4 0 1590.66 38.5663 2 1 4 0 1616.92 38.7871 1 2 -4 0 320.950 12.3370 1 2 -4 0 342.215 8.38887 2 -2 -4 0 349.707 9.04413 1 2 -4 0 326.429 10.5283 1 2 4 0 334.523 9.68128 2 2 4 0 341.909 9.41536 1 2 4 0 354.193 10.2297 1 -2 4 0 338.855 10.6567 1 -3 -4 0 147.355 4.76564 3 3 -4 0 153.698 6.07200 1 3 -4 0 158.745 7.92828 1 3 4 0 154.648 5.44550 2 -3 4 0 152.836 5.94199 1 3 4 0 149.666 5.57260 1 3 4 0 145.771 4.80553 1 4 -4 0 40.2778 2.90826 1 -4 -4 0 40.1187 2.08645 3 4 -4 0 40.0470 4.82081 1 4 4 0 36.1146 2.65155 1 4 4 0 38.1433 1.99321 1 4 4 0 42.4417 2.59696 2 5 -4 0 137.031 8.46916 1 5 -4 0 143.022 6.30531 1 -5 -4 0 147.975 5.14500 3 5 4 0 152.593 5.02285 1 5 4 0 145.022 6.30113 1 6 -4 0 858.341 27.8604 1 6 4 0 818.992 23.7618 1 6 4 0 791.680 21.3261 1 7 -4 0 100.485 8.11139 1 7 4 0 93.4619 5.98562 1 8 -4 0 -1.7463 2.51972 1 8 4 0 -0.5868 1.44762 1 0 -5 0 -4.9354 0.47705 1 0 5 0 -3.8037 0.85284 1 0 5 0 -4.4042 0.40287 2 -1 -5 0 2556.21 67.9727 1 1 -5 0 2532.72 66.0620 1 -1 5 0 2545.19 63.9339 1 1 5 0 2560.37 62.1651 2 -1 5 0 2556.14 64.0135 2 1 5 0 2667.71 62.6392 1 1 5 0 2426.25 63.4027 1 2 -5 0 6.02575 1.36575 1 2 -5 0 10.2369 2.64083 1 2 5 0 6.42568 1.33286 1 2 5 0 8.15516 1.18018 2 2 5 0 9.19132 1.25104 1 -2 5 0 7.63594 1.59403 1 3 -5 0 1120.98 30.5601 1 -3 -5 0 1172.61 28.5335 3 3 -5 0 1185.63 33.9330 1 3 5 0 1117.52 29.9336 1 3 5 0 1082.37 28.7079 1 3 5 0 1149.42 29.4245 2 4 -5 0 2117.13 54.3207 1 4 -5 0 2207.17 58.4793 1 -4 -5 0 2148.42 52.0840 3 -4 5 0 2040.21 53.5467 1 4 5 0 2078.14 53.7415 1 4 5 0 2135.45 52.2186 1 5 -5 0 80.7743 7.93254 1 -5 -5 0 81.5087 3.55083 3 5 -5 0 82.8630 4.79249 1 5 5 0 80.2157 3.52235 1 5 5 0 88.9614 4.91864 1 6 -5 0 221.957 12.1923 1 6 5 0 215.250 9.18156 1 7 -5 0 548.703 22.5827 1 7 5 0 562.641 18.7698 1 8 -5 0 83.8397 9.72914 1 8 5 0 77.9524 7.25601 1 0 -6 0 2459.14 61.4873 1 0 6 0 2507.34 62.8713 1 0 6 0 2489.21 60.5419 2 1 -6 0 2558.98 61.7744 1 -1 -6 0 2533.50 64.0421 1 1 6 0 2487.96 62.5966 1 -1 6 0 2430.06 60.0548 2 1 6 0 2455.61 61.4384 1 1 6 0 2390.99 60.7195 2 -1 6 0 2522.50 63.0605 1 2 -6 0 5428.36 138.185 1 2 -6 0 5631.33 133.184 1 2 6 0 5189.61 131.488 2 2 6 0 5014.58 131.111 1 -2 6 0 5306.91 128.616 2 2 6 0 5195.06 137.161 1 -2 6 0 5091.31 129.081 1 -3 -6 0 18.2399 1.64041 3 3 -6 0 17.2311 2.51762 1 3 -6 0 24.4413 4.20227 1 -3 -6 0 19.8437 1.27568 1 -3 6 0 19.6582 2.86212 1 3 6 0 20.1354 2.07356 1 3 6 0 16.4202 2.31792 1 3 6 0 22.0838 2.30252 2 4 -6 0 1162.65 35.8918 1 -4 -6 0 1152.39 29.2269 3 4 -6 0 1134.69 31.7368 1 4 6 0 1121.20 29.5465 1 4 6 0 1188.79 31.4996 1 -4 6 0 1145.81 31.4637 1 -5 -6 0 101.634 4.15103 3 5 -6 0 107.981 8.15191 1 5 6 0 100.215 5.60430 1 5 6 0 99.0826 4.27187 1 6 -6 0 46.8267 6.73124 1 -6 -6 0 49.2807 2.86139 3 6 6 0 43.6437 4.69404 1 7 -6 0 2.22985 2.45676 1 7 6 0 -1.2097 1.28064 1 8 -6 0 171.874 12.5679 1 8 6 0 162.116 9.10045 1 0 -7 0 -1.7402 0.57981 1 0 7 0 -1.0013 0.51799 2 0 7 0 -1.8595 0.88521 1 1 -7 0 966.978 25.7268 1 -1 -7 0 933.317 25.1470 1 -1 7 0 965.451 24.0381 2 1 7 0 932.827 26.7750 1 -1 7 0 930.785 27.0808 1 1 7 0 974.678 24.7664 2 -2 -7 0 932.872 24.5543 1 2 -7 0 909.472 25.6933 1 2 -7 0 953.570 30.4451 1 2 7 0 928.928 24.7937 2 2 7 0 956.324 25.2082 1 -2 7 0 960.043 27.1575 1 -2 7 0 936.187 23.3708 2 2 7 0 955.509 26.6402 1 3 -7 0 28.2224 5.03382 1 -3 -7 0 30.7319 1.84310 1 3 -7 0 30.9794 3.26860 1 -3 7 0 32.2400 3.87625 1 3 7 0 29.5726 3.31392 1 3 7 0 28.3209 2.23764 1 4 -7 0 209.315 11.9775 1 -4 -7 0 221.813 7.09211 3 4 7 0 218.096 7.61731 1 4 7 0 210.741 8.95546 1 -5 -7 0 54.7343 2.99908 3 5 -7 0 44.4016 6.53932 1 5 7 0 69.4541 4.83456 1 6 -7 0 15.2492 4.37743 1 -6 -7 0 12.8560 1.76227 3 6 7 0 13.8084 2.97490 1 7 -7 0 42.4173 7.32835 1 7 7 0 53.3965 5.84012 1 8 -7 0 136.023 13.5751 1 8 7 0 131.002 8.50811 1 0 8 0 182.207 6.19491 2 0 8 0 184.843 8.38187 1 1 -8 0 31.8154 2.67615 1 -1 -8 0 35.5798 2.63123 1 -1 8 0 29.3641 3.78620 1 -1 8 0 31.9930 1.91806 2 1 8 0 33.5045 2.82061 2 1 8 0 30.3968 3.71035 1 2 -8 0 340.678 11.4679 1 -2 -8 0 339.648 10.3468 1 2 8 0 330.785 12.2326 1 -2 8 0 335.560 9.19156 2 -2 8 0 318.042 12.4709 1 3 -8 0 42.6374 6.34203 1 -3 -8 0 34.2198 2.15382 1 3 -8 0 39.4055 3.82249 1 -3 8 0 42.0876 4.70768 1 3 8 0 37.4214 4.07637 1 3 8 0 30.6764 2.52740 1 -4 -8 0 29.7373 2.50090 3 4 -8 0 30.2105 3.44383 1 4 -8 0 31.1038 5.44626 1 4 8 0 35.8592 4.18420 1 -4 8 0 41.8168 4.63614 1 4 8 0 34.6612 2.68014 1 5 -8 0 46.7161 6.93471 1 -5 -8 0 45.0281 2.74082 3 5 8 0 41.1659 4.70622 1 6 -8 0 1.00467 2.29174 1 -6 -8 0 0.53020 0.70704 3 6 8 0 4.02930 1.78347 1 7 -8 0 5.47228 3.77879 1 7 -8 0 4.49530 1.94748 1 7 8 0 2.10476 2.29346 1 0 -9 0 -0.0880 0.63914 1 0 9 0 1.30072 1.29911 1 0 9 0 -0.0432 0.49013 2 -1 -9 0 49.4851 3.26569 1 1 -9 0 49.1157 3.46211 1 1 9 0 42.3347 4.58141 1 -1 9 0 55.0472 5.48419 1 -1 9 0 47.5580 2.52294 2 1 9 0 47.3183 2.91316 2 2 -9 0 -0.1767 0.68279 1 -2 -9 0 3.07416 0.96279 1 -2 9 0 -0.1678 1.05548 1 2 9 0 0.29096 1.02761 1 -2 9 0 1.45698 0.54453 2 -3 -9 0 65.3880 3.36125 1 3 -9 0 80.0246 4.81316 1 -3 9 0 64.4712 5.25885 1 3 9 0 67.8046 4.07956 1 3 9 0 66.9421 5.19262 1 -4 -9 0 271.302 8.72268 3 4 -9 0 264.826 14.9750 1 4 -9 0 266.070 10.5535 1 -4 9 0 258.330 11.5041 1 4 9 0 257.114 11.2469 1 5 -9 0 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9.06294 1 -1 -1 -9 71.2512 7.46820 1 1 -1 9 74.6993 12.0908 1 -1 1 -9 75.0965 7.85470 1 1 1 9 62.7713 11.1577 1 2 -1 9 35.8014 9.03837 1 2 1 9 42.0438 9.47286 1 5 -2 -9 706.565 23.8988 1 -5 -2 9 703.942 22.5862 2 -5 2 9 705.896 21.9937 2 5 2 -9 708.150 24.1937 1 -4 -2 9 120.223 7.01080 2 4 -2 -9 119.600 7.84067 1 4 2 -9 109.096 7.71803 1 -4 2 9 126.798 6.88667 2 3 -2 -9 253.990 12.1048 1 -3 -2 9 254.300 10.9560 2 3 2 -9 265.164 12.5357 1 2 -2 -9 72.8697 7.18637 1 -2 -2 9 57.1257 5.43795 2 2 2 -9 55.9899 6.36379 1 1 -2 -9 79.7077 7.63132 1 1 2 -9 61.2332 6.66587 1 0 -2 9 272.586 21.4191 1 0 -2 -9 269.746 13.2847 1 0 2 -9 291.188 13.8153 1 0 2 9 304.706 20.0835 1 1 -2 9 515.488 27.7991 1 -1 -2 -9 493.725 19.5759 1 -1 2 -9 496.856 20.0065 1 1 2 9 516.138 27.9177 1 2 -2 9 28.5870 8.54724 1 2 2 9 31.2840 8.83763 1 5 -3 -9 8.21145 2.77835 1 -5 -3 9 12.8429 2.86977 2 -5 3 9 8.22605 2.20318 2 5 3 -9 10.5114 3.12244 1 4 -3 -9 117.601 7.72331 1 -4 -3 9 112.860 6.84947 2 -4 3 9 122.500 6.74998 2 4 3 -9 114.091 7.96389 1 3 -3 -9 633.099 22.2282 1 -3 -3 9 637.666 20.8175 2 3 3 -9 617.350 22.4193 1 -2 -3 9 298.878 12.2698 2 2 -3 -9 324.074 13.9777 1 2 3 -9 290.943 13.7122 1 1 -3 -9 204.978 10.9858 1 -1 -3 9 225.174 10.1418 2 1 3 -9 220.059 11.6621 1 0 -3 -9 13.4578 3.36384 1 0 3 -9 13.8287 3.60194 1 0 3 9 11.2395 5.26845 1 -1 -3 -9 134.883 8.91568 1 1 -3 9 136.453 16.5650 1 -1 3 -9 130.756 9.21952 1 1 3 9 137.534 16.1830 1 2 -3 9 57.9377 11.4171 1 2 3 9 62.4442 11.4501 1 -5 -4 9 437.407 16.1957 2 5 -4 -9 431.380 16.9604 1 -5 4 9 419.703 15.0023 2 5 4 -9 447.608 17.4766 1 -4 -4 9 446.495 16.2636 2 4 -4 -9 455.619 17.4868 1 4 4 -9 459.865 17.8793 1 -4 4 9 426.411 15.4315 2 3 -4 -9 46.2577 5.67826 1 -3 -4 9 47.0376 5.02101 2 3 4 -9 40.1161 5.65007 1 2 -4 -9 91.3435 6.96789 1 -2 -4 9 97.8012 6.33938 2 2 4 -9 105.136 7.79381 1 1 -4 -9 6.87749 2.64230 1 -1 -4 9 10.0954 2.52809 2 1 4 -9 5.90062 2.69660 1 0 -4 9 1.27208 1.29835 2 0 -4 -9 0.86561 1.51657 1 0 4 9 0.13277 3.51399 1 0 4 -9 -1.1383 1.45510 1 -1 -4 -9 261.858 13.2802 1 1 -4 9 226.083 18.6566 1 -1 4 -9 298.145 14.4914 1 1 4 9 294.780 20.6048 1 2 -4 9 236.983 19.3875 1 2 4 9 236.791 22.6277 1 -4 -5 9 6.54715 2.15056 2 4 -5 -9 7.73585 2.62256 1 4 5 -9 10.0515 3.15736 1 -3 -5 9 13.1928 2.84294 2 3 -5 -9 18.9798 3.91731 1 3 5 -9 17.6504 4.03938 1 -2 -5 9 15.2316 2.94908 2 2 -5 -9 14.6565 3.50669 1 2 5 -9 9.45737 3.01558 1 1 -5 -9 1.34253 1.72877 1 -1 -5 9 5.33784 1.87166 2 1 5 -9 1.99916 2.10902 1 0 -5 9 3.10787 1.39674 2 0 -5 -9 1.83457 1.73675 1 0 5 9 -1.1684 2.91894 1 0 5 -9 0.77403 1.98846 1 1 -5 9 199.521 9.73031 2 1 -5 9 211.658 20.4161 1 -1 -5 -9 196.078 12.2589 1 -1 5 -9 193.978 11.7492 1 1 5 9 229.384 18.1120 1 2 -5 9 3.95246 5.16571 1 2 5 9 -4.2766 3.26713 1 4 -6 -9 238.616 12.0119 1 4 6 -9 253.548 12.7323 1 -3 -6 9 17.4242 3.25033 2 3 -6 -9 14.0831 2.34449 3 3 -6 -9 14.9467 3.41661 1 3 6 -9 14.4090 3.76273 1 -2 -6 9 1.62816 1.43581 2 2 -6 -9 -0.3654 1.45624 1 2 -6 -9 0.31289 1.02977 3 2 6 -9 -1.4357 1.48747 1 1 -6 -9 17.2335 3.76227 1 -1 -6 9 16.0982 2.95377 2 1 -6 -9 11.1475 2.38394 3 1 6 -9 14.6166 3.87884 1 0 -6 -9 13.5860 2.71904 3 0 -6 9 3.41723 1.81486 2 0 -6 -9 11.9390 3.25499 1 0 6 -9 9.50492 3.37506 1 0 6 9 7.62109 5.27203 1 1 -6 9 381.133 27.6048 1 1 -6 9 411.593 15.4272 2 1 6 9 423.541 25.2949 1 -1 6 -9 389.247 17.9020 1 4 -7 -9 12.8540 3.44075 1 4 7 -9 10.2885 3.45455 1 3 -7 -9 189.939 7.95271 3 3 -7 -9 187.677 10.4507 1 3 7 -9 174.163 10.8053 1 2 -7 -9 132.997 8.77178 1 -2 -7 9 146.098 9.13929 2 2 -7 -9 139.613 6.83468 3 2 7 -9 141.006 9.53662 1 -1 -7 9 61.7233 6.17529 2 1 -7 -9 78.4074 4.98749 3 1 -7 -9 67.0928 6.99649 1 1 7 -9 65.8320 7.66320 1 0 -7 -9 76.0929 5.33356 3 0 -7 9 90.2321 8.04310 2 0 -7 -9 78.4113 7.85414 1 0 7 -9 82.6051 8.72978 1 0 7 9 91.6178 19.0679 1 -1 -7 -9 357.592 13.4372 3 1 7 9 334.362 22.7088 1 -1 7 -9 325.195 16.4110 1 3 -8 -9 144.105 9.11539 1 3 -8 -9 135.684 6.71671 3 3 8 -9 139.676 9.71889 1 2 -8 -9 32.0712 5.11743 1 2 -8 -9 42.7114 4.29421 3 2 8 -9 52.3544 6.83912 1 1 -8 -9 163.702 7.88366 3 1 -8 -9 159.690 9.86516 1 1 8 -9 187.038 11.3961 1 0 -8 -9 49.6264 4.94609 3 0 -8 -9 36.7609 5.42346 1 0 8 -9 36.6131 5.98857 1 2 -9 -9 179.551 8.13871 3 2 -9 -9 162.477 10.1183 1 1 -9 -9 117.294 6.66762 3 1 -9 -9 127.785 8.77578 1 1 9 -9 121.722 9.48225 1 3 0 -10 671.537 24.5845 1 2 0 -10 660.670 24.4243 1 1 0 -10 199.829 11.5813 1 0 0 -10 11.3860 3.34867 1 3 -1 -10 38.1890 5.65082 1 3 1 -10 33.8099 5.37476 1 -3 1 10 36.7108 6.92149 2 2 -1 -10 85.2883 8.46942 1 2 1 -10 81.7386 8.35016 1 1 -1 -10 163.934 10.4940 1 1 1 -10 172.241 10.6530 1 0 -1 -10 126.040 9.14582 1 0 1 -10 115.329 8.82907 1 3 -2 -10 100.975 7.84006 1 3 2 -10 93.0241 8.89555 1 2 -2 -10 1.10141 2.00099 1 2 2 -10 0.15154 1.71319 1 1 -2 -10 26.1595 5.14539 1 1 2 -10 17.3078 4.24825 1 0 -2 -10 101.167 8.13988 1 0 2 -10 82.0384 8.67863 1 2 -3 -10 53.6722 6.86508 1 2 3 -10 60.6350 7.36939 1 1 -3 -10 0.55951 1.97762 1 1 3 -10 -0.8252 1.83267 1 2 -4 -10 94.0608 8.99372 1 1 -4 -10 5.46209 2.84895 1 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details 'SADABS 2014/4' _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_max 0.9485 _exptl_absorpt_correction_T_min 0.8815 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71070 7.125 15.271 8.198 89.994 99.990 90.020 ) ; _shelx_hkl_checksum 61804 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.55258(6) -0.15531(3) 0.11840(5) 0.01702(14) Uani 1 1 d . . . . . O1 O 0.72698(15) -0.06661(7) 0.46722(13) 0.0129(2) Uani 1 1 d . . . . . H5 H 0.6357 -0.0966 0.4889 0.019 Uiso 1 1 calc R U . . . O2 O 0.60124(15) 0.14869(7) 0.51730(14) 0.0164(3) Uani 1 1 d . . . . . N1 N 0.92146(19) 0.14972(8) 0.59019(17) 0.0151(3) Uani 1 1 d . . . . . H8 H 1.0307 0.1307 0.5677 0.018 Uiso 1 1 calc R U . . . C1 C 0.9231(2) 0.20661(12) 0.7324(2) 0.0223(4) Uani 1 1 d . . . . . H1 H 0.7921 0.2220 0.7422 0.034 Uiso 1 1 calc R U . . . H9 H 0.9945 0.2600 0.7180 0.034 Uiso 1 1 calc R U . . . H10 H 0.9836 0.1762 0.8331 0.034 Uiso 1 1 calc R U . . . C2 C 0.7611(2) 0.12520(10) 0.49254(19) 0.0129(3) Uani 1 1 d . . . . . C3 C 0.7849(2) 0.07034(10) 0.34414(19) 0.0137(3) Uani 1 1 d . . . . . H11 H 0.9200 0.0528 0.3542 0.016 Uiso 1 1 calc R U . . . H7 H 0.7521 0.1062 0.2427 0.016 Uiso 1 1 calc R U . . . C4 C 0.6614(2) -0.01126(10) 0.32650(18) 0.0115(3) Uani 1 1 d . . . . . H6 H 0.5264 0.0060 0.3278 0.014 Uiso 1 1 calc R U . . . C5 C 0.6719(2) -0.05788(10) 0.16592(18) 0.0123(3) Uani 1 1 d . . . . . C6 C 0.7668(2) -0.03313(10) 0.03947(18) 0.0136(3) Uani 1 1 d . . . . . H4 H 0.8407 0.0186 0.0410 0.016 Uiso 1 1 calc R U . . . C7 C 0.7403(2) -0.09470(11) -0.0936(2) 0.0194(4) Uani 1 1 d . . . . . H2 H 0.7946 -0.0880 -0.1908 0.023 Uiso 1 1 calc R U . . . C8 C 0.6297(2) -0.16376(11) -0.0670(2) 0.0192(4) Uani 1 1 d . . . . . H3 H 0.5991 -0.2110 -0.1422 0.023 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0220(2) 0.0152(2) 0.0138(2) -0.00174(13) 0.00293(17) -0.00310(15) O1 0.0122(5) 0.0153(6) 0.0114(5) 0.0027(4) 0.0022(4) -0.0008(4) O2 0.0116(6) 0.0167(6) 0.0212(6) -0.0028(4) 0.0039(5) 0.0002(4) N1 0.0112(7) 0.0157(7) 0.0183(7) -0.0048(5) 0.0019(5) 0.0015(5) C1 0.0185(8) 0.0236(9) 0.0241(9) -0.0117(7) 0.0013(7) 0.0013(7) C2 0.0144(8) 0.0094(7) 0.0154(7) 0.0018(5) 0.0041(6) -0.0008(6) C3 0.0146(8) 0.0131(7) 0.0136(7) -0.0003(6) 0.0032(6) -0.0015(6) C4 0.0112(7) 0.0121(7) 0.0110(7) 0.0006(5) 0.0013(6) 0.0003(5) C5 0.0109(7) 0.0121(7) 0.0132(7) -0.0003(5) -0.0002(6) 0.0010(5) C6 0.0132(7) 0.0153(8) 0.0117(7) -0.0013(6) 0.0000(6) 0.0007(6) C7 0.0188(8) 0.0275(9) 0.0121(7) -0.0009(6) 0.0035(6) 0.0029(7) C8 0.0223(9) 0.0205(8) 0.0135(8) -0.0047(6) -0.0006(7) 0.0024(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C8 S1 C5 92.53(8) . . ? C4 O1 H5 109.5 . . ? C2 N1 C1 122.54(13) . . ? C2 N1 H8 118.7 . . ? C1 N1 H8 118.7 . . ? N1 C1 H1 109.5 . . ? N1 C1 H9 109.5 . . ? H1 C1 H9 109.5 . . ? N1 C1 H10 109.5 . . ? H1 C1 H10 109.5 . . ? H9 C1 H10 109.5 . . ? O2 C2 N1 122.44(14) . . ? O2 C2 C3 121.64(14) . . ? N1 C2 C3 115.86(13) . . ? C2 C3 C4 112.86(12) . . ? C2 C3 H11 109.0 . . ? C4 C3 H11 109.0 . . ? C2 C3 H7 109.0 . . ? C4 C3 H7 109.0 . . ? H11 C3 H7 107.8 . . ? O1 C4 C5 111.24(12) . . ? O1 C4 C3 107.63(12) . . ? C5 C4 C3 110.80(12) . . ? O1 C4 H6 109.0 . . ? C5 C4 H6 109.0 . . ? C3 C4 H6 109.0 . . ? C6 C5 C4 128.90(14) . . ? C6 C5 S1 110.63(11) . . ? C4 C5 S1 120.47(11) . . ? C5 C6 C7 112.00(14) . . ? C5 C6 H4 124.0 . . ? C7 C6 H4 124.0 . . ? C8 C7 C6 113.18(14) . . ? C8 C7 H2 123.4 . . ? C6 C7 H2 123.4 . . ? C7 C8 S1 111.67(12) . . ? C7 C8 H3 124.2 . . ? S1 C8 H3 124.2 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C8 1.7090(17) . ? S1 C5 1.7268(16) . ? O1 C4 1.4425(17) . ? O1 H5 0.8400 . ? O2 C2 1.2449(19) . ? N1 C2 1.332(2) . ? N1 C1 1.454(2) . ? N1 H8 0.8800 . ? C1 H1 0.9800 . ? C1 H9 0.9800 . ? C1 H10 0.9800 . ? C2 C3 1.512(2) . ? C3 C4 1.520(2) . ? C3 H11 0.9900 . ? C3 H7 0.9900 . ? C4 C5 1.511(2) . ? C4 H6 1.0000 . ? C5 C6 1.385(2) . ? C6 C7 1.429(2) . ? C6 H4 0.9500 . ? C7 C8 1.358(2) . ? C7 H2 0.9500 . ? C8 H3 0.9500 . ?